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  • Ustinovshikov Jms 1993

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    IDhil Andi
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    The structure of an iron alloy containing 18% Cr and 0.72% n after different treatments was studied by x-ray and electron microscopy. Nitrogen provides a better combination of mechanical characteristics as well as higher fatigue strength, improved corrosion resistance and weldability of steels. The introduction.of a large quantity of nitrogen atoms into iron could decrease or completely exclude the employment of y-phase stabilizers such as nickel or manganese.

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    The structure of an iron alloy containing 18% Cr and 0.72% n after different treatments was studied by x-ray and electron microscopy. Nitrogen provides a better combination of mechanical characteristics as well as higher fatigue strength, improved corrosion resistance and weldability of steels. The introduction.of a large quantity of nitrogen atoms into iron could decrease or completely exclude the employment of y-phase stabilizers such as nickel or manganese.

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    13 visualizzazioni6 pagine

    Ustinovshikov Jms 1993

    Caricato da

    IDhil Andi
    The structure of an iron alloy containing 18% Cr and 0.72% n after different treatments was studied by x-ray and electron microscopy. Nitrogen provides a better combination of mechanical characteristics as well as higher fatigue strength, improved corrosion resistance and weldability of steels. The introduction.of a large quantity of nitrogen atoms into iron could decrease or completely exclude the employment of y-phase stabilizers such as nickel or manganese.

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    JOURNAL OF MATERIALS SCIENCE 29 (1994) 5489-5654 Non-stable structure of high-chromium and high-nitrogen iron-based alloy YU. USTINOVSHIKOV Physical Technical Institute of Russian Academy of Sciences, Izhevsk, Russia A. RUTS Udmurt University, Izhevsk, Russia 0. BANNYKH, V. BLINOV Baikov's Institute of Metallurgy, Moscow, Russia ‘The structure of an iron alloy containing 18% Cr and 0.72% N after different treatments was studied by X-ray and electron microscopy. It wes shown that the y-structure of the alloy after quenching is non-stable at all temperatures of isothermal holding, especially at high tempering ‘temperatures. The C-shaped hypothetical diagram of the alloy was constructed from the experimental results. 1. Introduction At the present time, there is 2 wide-spread tendency towards full or partial replacement of carbon by ni- trogen in steel. It is justified by the fact that nitrogen provides a better combination of mechanical charac- teristics as well as higher fatigue strength, improved corrosion resistance and weldability of steels. The replacement of carbon by nitrogen for steels contain- ing a large amount of chromium allows the formation of MasCe carbide to be avoided. The employment of nitrogen as an element forming interstitial phases is undoubtedly one of the prospective trends in the development of steels with improved propettis. Another prospective trend is t0 use nitrogen as a stabilizer of y-phase iron at room temperature, The introduction .of a large quantity of nitrogen atoms into ion could decrease ot completely exclude the employment of y-phase stabilizers such as nickel or manganese. In this case, however, ageing of nitrogen- containing iron-based alloys resulting in nitrides pre- cipitation” should be considered as an undesirable phenomenon promoting the ya transition, In order to shift‘the onset of nitrides precipitation to higher ageing temperatures it is possible to make use of the well-known properties of carbide- and nitride-forming, elements in steels, such as the delay of the onset of solid-solution decomposition, caused by them, ie. to use high-alloy steels, particularly high-chromium ones. The latter are known to have high corrosion resisting properties. It is rather difficult, however, to produce an austenite structure in high-chromium steels using nitrogen introduction, because chromium is an element which contracts the 7-region of iron in the phase diagram, In the present paper, results of the investigation of high-chromium steels are presented, where carbon is almost completely replaced by nitrogen. 022-2461 © 1994 Chapman & Hall 2. Experimental procedure The iron-based alloy containing 0.05% C, 18.0% Cr, 0.72% NN (impurities being in amounts within the standard for high chromium steels) was produced by melting armco iron and extralow-carbon ferrochrome in the laboratory furnace under a nitrogen pressure of, 1.8 MPa; the ingot was forged and homogenized. The forging was cut into the specimens for research. The specimens were exposed to different heat treatments: the varieties ofthe heat treatments arc indicated in the text and in the tables. The properties of the alloy after different modes of heat treatment have been deter- mined by measurement of the Rockwell hardness. The structure was investigated’ using transmission diffrac- tion electron microscopy. The quantity of y- and ‘o-phases in the structure. was measured by X-ray phase analysis. 3. Results and discussion The replacement of carbon by nitrogen in the high- chromium steel is not simply the replacement of one interstitial element by another, and thus the replace- ment of carbides by nitrides within the same struc- tures, but, in fact, itis the rearrangement of the whole phase diagram of the alloy. This may be seen in Table I, where the results on hardness measurements and X- determination of the y/a phase relationship after different modes of heat treatment are summarized. From the table it can be seen that after quenching from 900°C at any cooling rate, the hardness has high values (50 Hy. and even higher) and the structure represents 100% ferrite (the lattice parameter is about 0.2886 nm) having high ftagmentation and a high density of dislocations (Fig. 1). After quenching at any rate (into water, oil or air) from temperatures between, 5449 ‘TABLE [ Rockwall harness and relationship of and y-phases after quenching ‘Quenching parameters Rockwell y-pese in hardness structure (%6) 900°C, water, oil or alr 0 1150°C, water 8 150°C, of B33 130°C, air 5183s 200°C, water ae 200°C, 36-43 1250°C, 241 250°C, cil 32-36 250°C. aie Note: Some specimens were tested at every position Figure 1 Tae'strocture of bigh-temporature nitrous ferrite fer ‘quenching from 900°C, » 3600 1150 and. 1250°C, the structure is preferentially aus- tenite (Fig. 2) with the lattice parameter being equal to 03619 nm. The amount of austenite increases with heating temperature before quenching. It should be noted that there is no direct dependence between the amount of y-phase present in the structure, and hard- ness, ic. it is not possible to determine the amount of +y-phase from the hardness value, In addition, there is no direct dependence either between the heating tem- perature before quenching and the rate of cooling, on the one hand, and the y-phase amount, on the other. ‘The presence of 100% aephase in the structure after ‘quenching from 900°C could be explained by the fact that at relatively low heating temperatures before quenching, the CrN particles are not fully dissolved in the solid solution and the latter circumstance is dis- played on depletion of the solid by nitrogen; therefore, during quenching, the martensite y-« transformation of the depleted solid solution occurs, The trans- formation temperature is found to be considerably higher than room temperature. To verify this supposi- tion, several specimens were heated to 1150°C, held for 30min at this temperature, and further cooled, together with the furnace to 1050, 950, 850°C. Then they were held for 30 min at the above temperatures, taken out of the furnace and cooled in air. The results are given in Table Il. The presence of a large amount ‘yephase after quenching from 1130°C (Table 11) and the absence of any visible undissolved CrN particles, 5450 ‘gure 2 The structare of nitrous austenite ator quenching from 130°C; 36000. TABLE I Hardness and paso composition ater heating at 1150°C, cooling to temperatures given below and quenching in sit Quenching Rockwell ‘yeas in temperature CC) hardness structure (%6) us 3 37 1080 7 97 950 a a 850 st ° as is clearly seen in the electron micrographs (Fig. 2), suggests that all the chromium nitrides are dissolved in the solid solution at 1150°C. The same fact is evinced by the measurements of the lattice parameter of y-solation (0.3619 nm), the value of which corres- ponds to the Fe-18% Cr solid containing 0.72% N. ‘Two reasons could lead to the appearance of either amount of o-phase in the structure of the specimens quenched from 950 and 850°C: 1. fora temperature decrease from 1150°C down to 950 or 850°C, the 7-solid solution transforms into «through the +: intermediate region of the phase diagram and, during further quenching from 950 or 850°C, the structures of the high-temperature region of the phase diagram are fixed, ie. y + « of a3 2. on decreasing the temperature from 1150°C down to 950 or 850°C the CrN precipitation in y-solid ‘occurs, and therefore austenite is depleted by nitrogen, In the process of quenching the martensite y-< trans- formation occurs and a + CrN structure is fixed. ‘The experimental results, however, confirm the first supposition only. Firstly, the chromium nitrides are known to begin to dissolve in the solid on heating to relatively low temperatures, eg about 850°C [1] Secondly, the a-solid solution lattice parameter after quenching from 900°C is high enough, being 0.2885 nm, Supposing that chromium atoms influence inconsiderably the a-Fe lattice parameter and the introduction of 1 at% nitrogen increases the a-Fe parameter by 0.0008 nm, the conclusion may be drawn that if the lattice parameter is equal to 0.2885 nm, all the nitrogen remains in the solid solu- tion. The electron microscope data confirm this con= clusion (extra reflections from any CrN particles are completely absent after quenching from 900°C). The phase analysis indicates the absence of CrN particles in the anodic residue. Thus there is a rather wide region of a and ¥ co-existence in the phase diagram, approximately in the temperature range between 950 and 1250°C. To determine the initial point of the y-x martensite transformation, several quenched specimens were cooled to temperatures lower than room temperature. Other quenched specimens were kept at room temper- ature and somewhat higher temperatures to study the stability of the austenite structure. All the results are listed in Table II As was expected, at subzero temperatures, the par- tial transformation of nitrous austenite into ferrite cocours. The structure of such ferrite (Fig. 3) differs essentially from the ferrite structure formed after quenching from 900°C into water (Pig. 1). This fact shows that the mechanisms of the formation of these structures are different, and the a-phase structure fixed after quenching from 900°C and below, is not the product of y-a martensitic transformation, but repre- sents the structure of the a-phase existing at 900°C. The w-structure formed as the result of deep cooling of the quenched specimens, resulted from the ya trans- formation according to the martensitic mechanism. However, typical martensite structures characteristic, of carbon steels were not observed (Fig. 3) because the lattice of the Fe-Cr-N martensite is not tetragonal. On studying Fig. 3 one can see that the initial point of martensite transformation, M,, lies over the range 00 — 50°C. A certain increase of hardness and decrease of the amount of y-phase after the quenched specimen was kept for several days at room temperature, can be explained by nitrogen atom segregation processes at the boundaries, dislocations and other defects of the crystalline lattice of the alloy. Mittemeijer and Wierszyllowski [2], for example, have drawn the same conclusion concerning nitrogen-atom segregation at the crystalline lattice defects at low ageing temper- atures, Figure 3 The steucure of martensite afer holding the quenched alloy in liquid nitcogen; «26000. Similar segregation processes reduce the nitrogen concentration in the non-defect microzones of solid solution and the partial ya martensite trans formation seems to occur in those microzones. This process is accompanied by an increase in hardness of the alloy due to the growth of the coherent stresses at the austenite—ferrite boundaries. The nitrogen segre- Bation process at defects at room temperature is so slow that only 1%-4% of nitrous austenite transforms into ferrite over 4 days. Holding at higher temperatures (for example, at 100-300°C) leads to a certain increase in hardness and to the reduction of austenite in the structure (Table II, This process seems to be provided by inhomogeneity of the nitrogen-atom distribution in the 7-solid solution occurring at these temperatures, ice. by the same segregation processes as in the pre- vious case. It seems that decomposition of nitrous ferrite and nitrous austenite at the temperatures when diffusion mobility of substitutional atoms is suffi- ciently high, proceeds in different ways. Fig, 4 shows that the character of the hardness curves is different for ferrite and austenite decomposition. TABLE If Hardness and phase composition at subzero and low-temperature ageing of specimens queached from differen temperatures Quenching ‘Treatment Rockwell hardness phase in srvtore ( Parameers alter quenching Alter After Alter After quenching treatment quenching weatment 130°C, oi = 196°C, 1h 3 a 90 ” 130°C, oi = 50°C 3h 3 4 97 » 130°C, aie = 50°C. 3h 37 ae 97 66 130°C, oi + 20°C, 10 days 3 36 85 B 130°C, + 20°C, 10 days 3 3 » 37 LS0°C, oil + 20°C, 3 days) 23 0 100 160, 1150°C, ai + 20°C, 3 days 37 4 98 98 1200°C, aie 420°C, 10 days 36 8 a 87 180°C, oi 420°C, 3 days 3 x” 99 98 180°C, air + 20°C, 3 days 2 35 96 85 180°C, water 4100°C, Sh » a 100 » 1250°C, water 4+ 200°C, Sh 0 2 100 92 1280°C, water + 300°C, Sh 4 “4 100 50 080°C, water + 400°C, Sh 38 7 100 91 a 1 2 3 4 6 6 7 8 As-quenched ‘Ageing time (h) Figure 4 Rockwell hardness changes at sothermal ageing at dir cent temperatures: (J) austenite structure obtained ater quenching aged at 00°C; (2-4 ferrite structure obtained ater quenching aged 500, 550 and 600°C, respectively. Figure 5 Austerte strveture obtained after quenching aged at ‘500°C, 025 h, Dilfesion streaks in <100, directions « 6000, The decomposition of the alloy having austenite structure after guenching begins with nitrogen cluster formation and therefore, y > transformation in re- gions of the austenite depleted by N atoms takes place. X-ray phase analysis confirms that the ya. trans- formation occurs as only ageing temperature reaches, 500°C. With fonger ageing times (for cxample, 0.25 h) the highly dispersed regular structure, which is re- vealed due,to deformation contrast of the matrix, is observed (Fig. 5). This structure is characteristic of “alloys having high elastic coherent stresses, Appar- cently, these stresses arise in the coherent boundaries between precipitates. and matrix. Diffusion streaks paraliel to the [1 00] direction and associated with the (200) main reflection maximum are detectable in the lectron diffraction patterns (Fig, 5, inset). No addi- tional reflections of a new phase are observed. It can be supposed that the dispersed regular structure vis- ible in Fig. 5 does not seem to be new phase. pre- 5452 ipitates in the solid solution but represents mixed zones simultaneously enriched by chromium and ni- ‘trogen. Earlier, the analogous mixed zones of alloy clements atoms and carbon were observed during, secondary hardening of the alloy steels [3]. The structure at the peak of hardness represents particles of precipitates in solid solution (Fig, 6a). The particles lie on the (100), planes of the matrix, The electron diffraction pattern of this stucture is shown in, Fig. 6b. The orientation relationship of precipitate- ferrite was found to correspond to that originally proposed by Baker and Nutting for bcc and feo structures: (100), | (100), and [011], [001], (where p indicates precipitate, Fig, 6c). The electron i 202},-9 (002), Figure 6 (a) Austnit, structure obtained after quenching aged at 500°C, 2h peal of hardness, % 80000. (b) Electra difaction pattern fom (100), orientation; (c) schematic representation of () and n, reflections of two nitride systems. Jiffraction pattern and its identification in Fig. 6 show that particles of precipitates at the-peak of hardness are CN having fee structure of NaCl type with a lattice parameter of 0.414 nm, Elastic distortions of the matrix at the boundaries between it and pre-

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